金属材料分析方法的选择和施行：第五讲 金属材料中钨的测定（续）

此外,尚有二硫酚、邻羟基酚类试剂、酸性三苯甲烷类试剂、偶氮类试剂以及荧光酮类试剂等也都有应用于钨的光度测定的实例。但由于共存元素的干扰以及方法的成熟程度等问题尚未完全得到解决,在金属材料分析中的应用尚不普遍。其中,苯基荧光酮类试剂对钢铁中低含量钨的测定有一定的应用前景,举两例说明:例1:邻氯苯基荧光酮(o-Cl-PF)-CTMAB光度法测定钢及合金中低含量钨[w(W)0.01%~0·50%]。称取试样0.100 0~0.200 0 g,溶于硫酸-磷酸混合酸(H2SO4+H3PO4+H2O=3+10+12)10 mL中,滴加浓硝酸约1 mL氧化,蒸发至冒白烟,冷却,加水溶解盐类后冷…     

Radiation Effects on Concentrated Potassium Hexacyanoferrate(III) Solutions

The neutron irradiated potassium hexacyanoferrate(III) solutions were analyzed for Fe(CN)₆^4?, Fe(CN)₆^3?, and Prussian blue. The retention values (1.1%) were constant throughout the pH and concentration ranges studied, and did not change with the length of irradiation. The complex behavior of the radiochemical yield of the Fe(CN)₆^4? and Prussian blue was attributed to the competition of the various reactions involved in the irradiation.     

三磷酸胞苷在Duolite A-30树脂上的交换过程研究

根据CTP在离子交换树脂上的吸附容量和分离因数的大小,确定Duolite A-30树脂适合CTP与CDP,CMP之间的分离.对CTP在Duolite A-30树脂上的吸附动力学和热力学研究表明,在283.15K~303.15K之间,CTP的质量浓度在7.5g/L以上时,Duolite A-30树脂对CTP的吸附主要受颗粒扩散的控制,其有效扩散系数为D=3.47×10-7cm2/s,溶液的质量浓度≤1.0g/L时,CTP与Duolite A-30树脂之间的交换速率主要受液膜控制,其液膜扩散系数为Kf =4.112×10-4/s.同时测定了不同条件下三磷酸胞苷溶液在Duolite A-30树脂固定床离子交换柱中的穿透曲线,研究了进口浓度、进口流速、原料液温度、原料液的pH值及柱高对穿透曲线的影响.用二阶动力学推动力模型描述固定床动态过程,考察了轴向返混对穿透曲线的影响,并从穿透曲线回归得到总传质系数,模型计算值与实验数据符合良好.     

Pulsed photothermal phase-shift spectroscopy for weak absorption measurement

A novel photothermal phase-shift spectroscopy configuration based on the retro-reflected beam interference has been developed and its operational principle is described. The weak absorption measurement ability of this technique is experimentally proven with a water/ethanol solution of standard Pyronine G dye and the limit of detection is found to be 1.8 x 10(-6) absorbance. Potential applications of the technique are discussed.     

Preparation of Y2Ba4Cu7O15-δ Superconductor without High Oxygen Pressure

The synthesis of bulk Y₂Ba₄Cu₇O_15-δ superconductor at atmospheric oxygen pressure via solid state sintering is reported. Temperature ranging from 860 to 890 °C as well as time interval over 2 to 15 days were used to investigate the formation of the Y₂Ba₄Cu₇O_15-δ phase. A time-temperature profile characterizing the conditions for the preparation of Y₂Ba₄Cu₇O_15-δ phase suggests the optimal condition to be sintering at 890 °C for over 10 days. Detailed results of X-ray diffraction, electrical resistivity, iodometric titration and magnetization measurements are described.     

果蔬中L—抗坏血酸的示波计时电位K3Fe（CN）6滴定法研究

本文报导的方法是在南京大学高鸿教授研究的K_3Fe(CN)_6示波极谱滴定法(在PH8的K_2HPO_4—KH_2PO_4—KBr底液中,用0.04660mol/LK_3Fe(CN)_6标准溶液对纯抗坏血酸测定)的基础上,考虑到L—抗坏血酸(以下简称V_e)在碱性、中性介质中稳定性差,如用于V_e含量很微的果蔬测定,对结果影响大。本文改为H_2C_2O_4—KBr的酸性介质作底液,用     

人工神经网络X射线荧光光谱法测定钢中酸溶铝

建立了一种人工神经网络-X射线荧光光谱法测定钢中酸溶铝的方法，用X射线荧光光谱法测定低合金钢中总铝值，应用所建立的ANN-BP网络模型，输入总铝含量直接预测出酸溶铝含量。同时使用改进的BP算法，避免了神经网络学习中可能产生的麻痹现象。该方法用于钢中酸溶铝的测定，结果满意。     

探针反应和FTIR法研究Pt与L型沸石的相互作用

探针反应和ＦＴＩＲ法研究Ｐｔ与Ｌ型沸石的相互作用董家禄,朱建华,须沁华,张婕,刘大壮（南京大学化学系,南京,２１０００８）（郑州工学院化工系,郑州,４５０００２）关键词Ｐｔ／Ｌ沸石,沸石催化剂,异丙醇分解反应,Ｐｔ－载体相互作用Ｐｔ的分散度和电子状态...     

Enantioselective Addition of Iodine Azide to α,β-Unsaturated Carboxylic Acid Derivatives

The addition of iodine azide to chiral conjugated N-enoyl-sultam or α,β-unsaturated N-acyloxazolidinones generated two asymmetric centers at C(α) and C(β) with high π-face differentiation and regioselectivity. The diastereomerically pure product was easily obtained by crystallization with purity up to 94% de. The structure of 2a was determined by X-ray diffraction analysis which also indicated that B and 4 are reactive conformations.     

Synthesis of 8,9-dialkoxy-substituted tetrahydrobenz[h] isoquinolines

6,7-Dimethoxy-2-naphthylethylamine, prepared by the diborane reduction of 6,7-dimethoxy-2-naphtlialeneacetamide, underwent a Pictet-Spengler cyclization to form 8,9-dimethoxy-1,2,3,4-tetrahydrobenz[h]isoquinoline. This compound is identical with that obtained by reduction of the corresponding dihydrobenzisoquinoline prepared from formamide cyclization. 6,7-Dialkoxy-2-naphthaleneacetic acids, the key intermediates for the preparation of these amides, were obtained from 6,7-dialkoxy-2-acetonaphthones by a modified Willgerodt reaction.